分散液液微萃取和气质联用测定葡萄酒中的主要高级醇  

Determination of higher alcohols in wine by dispersive liquid-liquid microextraction(DLLME) and gas chromatography-mass spectrometry

作　　者：倪伟[1] 周志磊[1] 姬中伟[1] 刘双平[1,2] 韩笑 毛健[1,3,4] NI Wei;ZHOU Zhi-lei;JI Zhong-wei;LIU Shuang-ping;HAN Xiao;MAO Jian(National Engineering Laboratory for Cereal Fermentation Technology, Synergetic nnovation Center of Food Safety and Nutrition, School of Food Science and Technology Jiangnan University, Wuxi 214122;Jiangsu Industrial Technology Research Institute （Rugao Jiangnan University Food Biotechnology Research Co., Ltd.）, Rugao 226500;Jiangnan University （Rugao） Food Biotechnology Research Institute, Rugao 226500;National Engineering Research Center of Chinese Rice Wine, Shaoxing 312000)

机构地区：[1]江南大学食品学院粮食发酵工艺与技术国家工程实验室江南大学食品安全与营养协同创新中心,无锡214122 [2]江苏省产业技术研究院食品生物技术研究所(如皋江大食品生物技术研究所有限公司),如皋226500 [3]江南大学(如皋)食品生物技术研究所,如皋226500 [4]国家黄酒工程技术研究中心,绍兴312000

出　　处：《食品科技》2018年第6期283-291,共9页Food Science and Technology

基　　金：国家自然科学基金项目(31571823);江苏省自然科学基金项目(BK20161293);国家重点研发计划项目(2017YFD0400103);北京工商大学食品营养与人类健康高精尖创新中心开放基金项目(20161041);北京工商大学食品质量与安全北京实验室开放课题

摘　　要：高级醇是酒精饮料中重要的风味化合物。建立了一种基于分散液液微萃取(DLLME)结合GC-MS测定葡萄酒中4种主要高级醇的方法。通过优化样品酒度、pH、萃取剂、萃取剂体积、分散剂、分散剂体积、样品体积、盐浓度和萃取时间,获得了最佳的DLLME参数:样品酒度12%vol以下,pH和离子强度无需调节,800μL二氯甲烷作为萃取剂,1.0 mL乙腈作为分散剂,7 mL的葡萄酒样品,提取时间1 min。方法的相关系数(r)为0.9907~0.9994,均大于0.99。检测限(LOD)为(0.09~0.75)mg/L,定量限(LOQ)为(0.32~2.49)mg/L,均低于葡萄酒中的浓度。RSD均低于4.5%,重复性良好。利用该方法对不同甜型的成品葡萄酒中的高级醇进行加标回收,回收率为81.57%~111.15%。Higher alcohols are important flavor compounds in alcoholic beverages. A new method for determination of the main higher alcohols was developed based on dispersive liquid-liquid microextraction（DLLME） coupled with GC-MS. Wine was selected as an example to develop the method and the optimal DLLME parameters were acquired： the sample ethanol concentration were diluted to 12% vol, no pH adjustment was required, 800 μL dichloromethane as extraction solvent, 1.0 mL acetonitrile as dispersant, 7 mL of wine sample, 1 min of extraction time and no salt addition. The performance of the method was satisfactory. The correlation coefficients（r） ranged from 0.9907 to 0.9994. The LOD was between 0.09 mg/L and 0.75 mg/L, the LOQ ranged between 0.32 mg/L and 2.49 mg/L and lower than the concentration of higher alcohols in wine. The RSD was lower than 10% and the recoveries were from 81.57% to 111.15%.

关 键 词：分散液液微萃取 高级醇 葡萄酒 GC-MS 

分 类 号：TS207.3[轻工技术与工程—食品科学]